Process for preparation of

ABSTRACT

A PROCESS FOR PREPARING 2,2-DIALKYLPROPANE-1,3-DIOLS BY CONTACTING AN ALCHOLIC SOLUTION OF AN ALDEHYDE HAVING A SINGLE ALPHA-HYDROGEN ATOM AND FROM 5 TO 23 CARBON ATOMS WITH FORMALDEHYDE IN THE PRESENCE OF A CAUSTIC ALDOL CONDENSATION CATALYST. THE ALDEHYDE IS PRESENT IN A RATIO OF FROM 1 TO 3 MOLES OF ALDEHYDE PER MOLE OF FORMALDEHYDE. THE REACTION IS CONDUCTED AT A TEMPERATURE OF FROM 0* C. TO 40* C. TO FORM AN ALDOL. THE ALCOHOL, SALTS AND CATALYST RESIDUE ARE REMOVED BY WATER WASHING. OTHER DISSOLVED IMPURITIES AND UNREACTED RE-   AGENTS ARE REMOVED BY STRIPPING WITH A HEATED INERT GAS. THE PURIFIED ALDOL IS REDUCED WITH HYDROGEN IN THE PRESENCE OF A BARIUM-PROMOTED COPPER-CHROMIUM OXIDE CATALYST AND SUBSEQUENTLY STRIPPED OF REDUCTION BY-PRODUCTS WITH AN INERT GAS TO YIELD THE ESSENTIALLY PURE DIOL.

DEFENSE/E PULlGATlN UNITED STATES PATENT OFFICE Published at the request of the applicant or owner in accordance with the Notice of Dec. 16, 1069, 869 O.G. 687. The abstracts of Defensive Publication applications are identified by distinctly numbered series and are arranged chronologically. The heading of each abstract indicates the number of pages of specification, including claims and sheets of drawings contained in the application as originally filed. The files of these applications are available to the public for inspection and reproduction may he purchased for 30 cents a sheet.

/ Defensive Publication applications have not been examined as to the merits of alleged invention. The Patent Oflice makes no assertion as to the novelty of the disclosed subject matter.

PUBLISHED NOVEMBER 30, 1971 nmzmrm: srnwpma COLUMN 7 HEAT 4 mums I g cxrmcno COLUMN (I z SOLVENT necevsm newt-m g PRODUCT :aLuuN PUMP ' g ALCOHOL cowl-m A process for preparing 2,2-dialkylpropane-1,3-diols by contacting an alcoholic solution of an aldehyde having a single alpha-hydrogen atom and from 5 to 23 carbon atoms with formaldehyde in the presence of a caustic aldol condensation catalyst. The aldehyde is present in a ratio of from 1 to 3 moles of aldehyde per mole of formaldehyde. The reaction is conducted at a temperature of from 0 C. to 40 C. to form an aldol. The alcohol, salts and catalyst residue are removed by Water washing. Other dissolved impurities and unreacted reagents are removed by stripping with a heated inert gas. The purified aldol is reduced with hydrogen in the presence of a barium-promoted copper-chromium oxide catalyst and subsequently stripped of reduction by-products with an inert gas to yield the essentially pure diol.

Nov. 130, 1971 PROCESS FOR PREPARATION OF 2,2-DIALKYLPROPANIl-fl.,5-DIOL H. J. AGEMEYER, JR., L

Original Filed May 27, 1968 Nwmoo 'IOHOCHV 5'2" NWFIIOO SNIddIHlS SHEIIOS MO'I HOLOVEIH NWI'TIOO SNIddIHiS HGAHBG'IV AT ORNEYS 

